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HCID 86736134、化合物 → HCID 20377673、化合物

HRID 2052362
ノート
印刷プレビュー

反応式

HRID 2052362 の反応式
[S:1]1[C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=[C:2]1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([C:17](C)([C:23]([O-])=O)[C:18]([O:20]CC)=[O:19])=[CH:13][CH:12]=1)=[O:10]>[OH-].[Na+].C(O)C.O>[S:1]1[C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=[C:2]1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([CH:17]([CH3:23])[C:18]([OH:20])=[O:19])=[CH:13][CH:12]=1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 86736134HCID 86736134、化合物

生成物 1

HCID 20377673HCID 20377673、化合物収率 74.7%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Ethyl 2-{4-(thieno[2,3-b]thien-2-yl)carbonyl-phenyl}-2-methyl-malonate (16.23 g) is suspended in a mixture of 5% (w/v) aqueous sodium hydroxide solution (90 cc) and ethanol (90 cc), and the suspension is heated at the boiling point for 3 hours. After cooling, the reaction mixture is diluted with distilled water (1000 cc), and then extracted three times with diethyl ether (total 600 cc). The aqueous phase is filtered off, acidified to pH 1 by the addition of a 5 N aqueous hydrochloric acid solution and extracted three times with diethyl ether (total 600 cc). The combined ether solutions are washed three times with distilled water (total 300 cc), dried over anhydrous sodium sulphate, decolourizing charcoal (1 g) is added, and the solutions are filtered and evaporated. Crude 2-{4-(thieno[2,3-b]thien-2-yl)carbonyl-phenyl}propionic acid (9.9 g), melting at 150° C., is thus obtained.

後処理

  1. temperaturethe suspension is heated at the boiling point for 3 hours
  2. temperatureAfter cooling
  3. extractionextracted three times with diethyl ether (total 600 cc)
  4. filtrationThe aqueous phase is filtered off
  5. additionacidified to pH 1 by the addition of a 5 N aqueous hydrochloric acid solution
  6. extractionextracted three times with diethyl ether (total 600 cc)
  7. washThe combined ether solutions are washed three times with distilled water (total 300 cc)
  8. dry with materialdried over anhydrous sodium sulphate
  9. additionis added
  10. filtrationthe solutions are filtered
  11. customevaporated

出典と根拠

ORDレコード
ord-8e965d1092394dec93bebb821f2539cf
出典データセット
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04183944

反応ノート

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